Apparatus for liquefying chlorine gas



W. M. JEWELL APPARATUS FOR LIQUEFYING GHLQRINE GAS March 31, 1925 Filed March 13, 1920 ZSheets-Sheet 1 W. M. JEWELL APPARATUS FOR LIQUEFYING CHLORINE GAS March 31, 1925- Filed March 13,1920 2 Sheets-Sheet 2 Patented Mar. 31, 1925.; I

UNITED STATES JPAITENTN OFFICE.

WILLIAM H. JEWELL, OF CHICAGO, ILLINOIS, ASSIGNOR TO CHLORINE PRODUCTS COMPANY, OF CHICAGO, ILLINOIS, A CORPORATION 01 ILLINOIS.

APPARATUS FOR LIQUEI'YING CHLOBINE GAS.

Application filed March 13', v19130. Serial No. 365,898.

To all whom, it may concern:

Be it known that I, WILLIAM M. JEWELL,

a citizen of the United States, residing at 720 N. Lotus Ave, Chicago, in the county of Cook and State of Illinois, have invented a new and useful Improvement in Apparatus for Liquefying Chlorine Gas, of which the following is a specification.

The manufacture of liquefied chlorine as, by apparatus hitherto provided, invo ves what is known as mechanical refrigeration for reducing the temperature of the condensers for the compressed gas to a relatively low temperature, commonly in the neighborhood of 35 F. below zero, in order to avoid the com ressing of the gas to very high pressure. uch a paratus also involve the subjection of the old orine gas to chemicals to separate the gas from air, hydrogen and other gaseous ingredients it may contain, as by the use of a solvent such as carbon-tetra-chloride, and the subsequent distillation of the chlorine as by steam, recooling, or'chilling of the c ilorine distillate, the recovery of the solvent for further use, or the use of slow-operating earthenware pumps or high entrainment towers for compressing the chlorine gas and auxiliary apparatus for absorbing the uncondensable portion of the chlorine with quick lime, or other suitable chemical, all of which results in complicated and expensive plants which are troublesome to maintain in proper working condition. 7

Furthermore. it has been the practice, owing to the fact that theli uid chlorine upon being discharged from t o condenser is at a relatively low temperature, as, for example, 35 F. below zero, to employ a relatively large receiving tank into which the chlorine flows, and in which tank-the liquefied chlorine is permitted to remain until the temperature thereof approximates the temperature of the atmosphere surrounding the tank, from which latter the shipping cylinders or containers,are filled, this condition also causing the apparatus to be expensive of construction and expensive to operate, and rendering the operation of the apparatus intermittent.

My primary object is to so improve upon apparatus previously employed that chlorine gas may be liquefied at a greatly reduced expense, both from the standpoint of cost of apparatus required to be used and the cost of operating the same, and generally to ren er easier and less costly the production of substantially pure liquefied chlorine.

Referring to the accompanying draw- Figure 1 shows by a view, in the nature of a diagram, an ap aratus constructed in accordance with my invention; Figure 2 is a perspective view of a as compressor employed, with a ortion o the crank case of the compressor roken away to disclose interior details; Figure 3 is a view like Fig. 1 of a variation in the portion of the apparatus shown in this figure; and Figure 4, a section taken at the line 4-4 on Fig. 3 and viewed in the direction of the arrow, with coil omitted.

Referring more particularly, to the apparatus disclosed in Figs. 1 and 2, a pipe, represented at 3, leads from the apparatus wherein the chlorine gas is produced, as, for example, from an electrolytic cell or cells (not shown) and which operate to produce electrolytic chlorine gas which commonly contains some non-condensable gas, this pipe connecting with the upper end of a coil 4 of a cooling apparatus 5, this coil being contained in a chamber 6 through which a cooling medium, as, for example, water, is circulated, the water entering the bottom of the tank 5 through the pipe 7 and discharging therefrom at its top through the pipe 8. The lower end of the coil 4 connects with a trap 9 in the form of a U-pipe communicating at its lowest portion witha pipe 10 through which condensable matter removed from the chlorine gas in'the coil 4, is withdrawnthrough the outlet pipe 11. The trap 9 connects with a pipe 12 which opens into the bottom of a preliminary drying tower 13 which may be of any suitable construction, the same being shown as of the loose-packing type, as represented at 14, whereby the gas flowing into the dryingtower is caused to pass in a zigzag course to the upper portion thereof from which it passes through a pipe 15 which connects with the lower end of another drying tower 16 which may be of the same general construction as described of the tower 13, the gas passing upwardly through the tower 16 and passing therefrom through a pipe 17 which connects with a coil 18. The coil 18 as shown is jacketed by the coil 19 having an inlet pipe and an outlet pipe 21,this part of the apparatus being so constructed that chlorine gas with acid therein, as hereinafter explained, will pass through the coil 19 in a direction contrary to the flow of gas throu h the coil 18. The end of the coil 18 opposite that connected with the pipe 17 is provided with a valve 22 and connects with the inlet opening of the compressor represented at 23, a pipe 24 communicating with the outlet opening in the cylinder of the compressor for the compressed gas. The compressor 23 may be of any suitable type, that shown being a common and well-known construction of compressor of the reciprocating type, the crank case thereof being represented at 25 and in which the lower end of the connesting rod 26 of the compressor-piston operates, as shown in Fig. 2, the compressor shown being operated from the shaft 27, as by an electric motor 100 belted to a pulley 101 on the shaft 2'7. l'n the use of the compressor, its piston (not shown) is lubricated by means of comparatively dry sulphuric acid, the acid by preference being at least of 1.84 specific gravity at 66 Baum 95% pure, and to accomplish this, the acid may be supplied to the interior of the crankcase 25 from which it becomes supplied to the piston for lubricating the latter in its movements in the cylinder, by the action of the connecting rod 26 and its connection with the crank shaft 27 operating as a splash feed. In the particular apparatus shown, the sulphuric acid is supplied to the crank-case 25 through a pipe 28, valved as indicated at 29, and connected with the lower end of a tank 30 shown as supported at 31 and communicating by a pipe 32, valved at 33, with a supply of sulphuric acid. The upper end of the tank 30 connects by a pipe 34 with the pipe 20, the pipe 34 adjacent the tank 30 having a branch 35 provided with a vent-valve 36 which is opened to permit the gas pressure in the chamber 30 to vent therefrom during the filling of this chamber with the acid. The crank-case 25 contains an outlet about midway between its top and bottom for the sulphuric acid which connects with a pipe 37 opening into a trap communicating with a pipe 40 which opens into the drying tower 13 and terminates above the packing 14 therein, in a spray-head 41 for spraying sulphuric acid against the rising currents of chlorine gas passing upwardly through the tower. The compressor-outlet pipe 24 contains a valve 42 and opens into the upper end of a tank 43 of a cooling apparatus 45 the coil of which, for the cooling medium, and which is located in the tank 43, being represented at 44. A pipe 46 for cooling water supplied thereto as hereinafter described, connects with the upper end of the coil 44 for causing cooling water to flow through the latter from which it discharges through 9. pi e 47 into the jacketed portion of the cylindbr 48 of the compressor, the outlet of this jacketed portion being represented at 49 and o ening into a sewer.

A pipe 51 lea ing from a supply (not shown) of cooling water connects with the upper end of a coil 52 which lies in the bottom of the crank-case 25, the outlet of this coil communicating with a pipe 53 which connects with a condenser hereinafter referred to.

The lower end of the tank 43 opens into the pipe 20 through which liquid chlorine with some of the sulphuric acid passes for the purpose above stated.

The outlet of the tank 43 for this com pressed chlorine gas connects with a pipe 54 valved, as indicated at 55, and formed into a coil as represented, this coil being surrounded by a coil 56 connected at its lower end with a valved water-inlet pipe 57 which connects with the pipe 53, the upper end of the coil being connected with the pipe 46, the coils 54 and 56 forming a condenser in which the cooling water travels in a direction contrary to the flow of the gas. A. pipe 54* preferably connects with the pipe 54 and has branch pipes 54 and 54, the pipe 54 being equipped with a gauge 54 and the pipe 54 which forms a vent-pipe, being equipped with a valve 54 A pipe 58 valved at 59 leads from the coil 54 to a "l'-coupling 60 one outlet of which connects with a pipe 61 connected by a flexible pipe 61 with a pipe 61 which terminates in a hollow head 52 with a valve 63, this head being connected with the inlet of a shipping container represented at 65, the container shown being such as are commonly used and holding about pounds of liquid chlorine, the container being enclosed in heat-insulating material represented at 66 and shown as supported on a weighing scale 70. lhe other outlet of the T-coupling 60 connects with a pipe 67 having an enlargement 68 with a valve '59 below the enlargement, this pipe opening into the upper end of the drying tower 16'and terminating therein in a sprayhead (not shown) for spraying sulphuric acid, separated in the chamber 68 from the liquid chlorine, into' the chlorine gas as it passes upwardly through this tower.

In the operation of the apparatus as shown, the chlorine gas is drawn from the electrolytic cells hereinbefore referred to, by a slight vacuum preferably of about to of water, produced by the action of the compressor and regulated by the valve 22, the gas with its contained water-vapor, which is present to a considerable degree and which should be removed, passing through the pipe 8 into the coil 4 wherein it is subjected to the cooling action of the water flowing into the latter through the lihl pipe 7 and flowing out by the pipe 8, wherem the larger part of the water vapor in the gas is condensed and separated from the gas in the trap 9, the water thus separated Y flowing off throu h the outlet-pipe 11. The

gas thus partial y freed of its contained moisture then flows into the dr ing tower 13 wherein further drying is e ected by the rising currents of the gas contacting the packing 14 which is wetted by the discharge of acid against it, the acid being supplied through the spray-head 41 from the pipe 40, trap 38, pipe 37 and crank-case 25, the

- drying tower 16 through which latter it upwardly passes in contact with the acking 14 wetted with a shower of sulp uric,

acid from the spray-head (not shown) but hereinbefore referred to and supplied with sulphuric acid from any suitable source, supplemented by sulphuric acid which passes into the pipe 67 from-the separator chamber 68, the moisture in the gas being reduced thereby to about 0.3 to 0.5 milligrams per liter, the final drying of the gas taking place in the tower 16. The gas then passes through the coil 18 where it. is subjected to the cooling action of expanding chlorine gas which 1s supplied to the coil 19, to flow in a direction therethrough opposite to the flow of the gas through the coil 18, from the chamber 43 through the pipe 20. The gas in cooled condition then passes through the valved pipe 18 into the inlet of the compressor w lere it is compressed to about 100 pounds per square inch and in the compressing operation is commingled with sulphuric acid in finely divided condition and preferably partially vaporized, the acid being fed to the piston for lubricating it by the splash-feed action of the connecting-rod 26 operating in the crank-case 25 which contains sulphuric acid supplied thereto as stated. The com ressed gas, together with some of the aci commingled therewith as stated, discharges from the compressor through the valved pipe 24, and thence into the upper end of the tank 43 of the cooling apparatus 45' which operates as a trap, where it is subjected to the coelin' action of the water which entersthe coi 44 therein from the pipe 46 and discharges through the pipe 47 into the jacket of the compressor to grevent overheating of its cylinder 48. on-

densing of a portion of the chlorine and sulphuric acid 1s effected in the tank 43, the acid being heavier than the li uid chlorine gravitatin to the bottom of t is tank and flowing with chlorine through the pipe 20 and coil 19 back to the crankcase 25. The chlorine either as gas or liquid passes from the tank 43 through the pipe 54, which preferably is located a considerable distance from the bottom of the tank 43, into the condenser 54 which completes the condensing of the chlorine gas which passes over from the cooling tank 45, the chlorine in passing through the condenser. 54 being subjected to the cooling action of the oppositely flowing currents of cold water in the coil 56. The condensed chlorine and any condensed sulphuric acid content, discharges into the pipe 58, the acid settling in the chamber 68 and the li uid chlorine entering the pipe 61 from which the chlorine, which is substantially 100% pure, ma y be filled into the shipping containers such, for example, as the one shown at 65. The effect of operating on the chlorine as described is to produce in the condensing apparatus beyond the compressor, liquefied chlorine at a temperature of the coil 54 of approximately F. and under relatively low pressure as stated, thus permitting the liquefied chlorine to be directly charged into the shipping containers. In the filling of the containers the air is, by preference, exhausted therefrom before the filling operation begins, this exhausting operation being effected in any desired manner. The container is preferably first cooled to a point below the temperature of the condensed chlorine and then enclosed in the insulating covering 66 and thereupon the air exhausted from the container. The container is then connected with the pipe 61 and the liquid chlorine thenpermitted to flow into the container, this filling operation being quickly effected. The insulating of the container 65 serves to keep down the gas pressure in the coil 56 and this is further facilitated by permitting a portion of the liquid chlorine in the container 65 to evaporateby closing the valve 59 and opening valve 69. The gas thus liberated, together with the accumulations of acid in chamber 68, flows back through pipe 67 to the tower 16 and is thus not wasted. The temperature of the containers may thus be caused to be less than the temperature of the water in the condenser coil 56 so that no additional gas pressure is required for filling the containers.

The efi'ect of causing the compressed chlorine gas and sulphuric acid to become commingled, is to render the compressed chlorine gas condensable at such a relatively high temperature that the chlorine gas may even though quite impure and compressed only to temperature conditions permit; and

the relatively low degree of substantially 100 pounds to the square inch, be condensed at relatively high temperature, as for example F., the temperature of ordinary water, with the manifest advantages, especially over prior practices involving the refrigeraation of the compressed gas to temperatures at, or approximately at 35 F. below zero. While I the purpose stated, if desired, other substances condensable at higher temperatures than that at which pure chlorine under the same pressure condenses, may be used and the commingling of such substance and the gas, accomplished in any desired way, as also the commingling of the sulphuric acid and the gas may be effected in other ways than that described.

The feature of maintaining a pressure of chlorine gas in the crank-case is of advantags as thereby the suction action'produced by the operating parts of the compressor is not exerted on the surrounding atmosphere, but is neutralized by the pressure in the crankcase and thus no air which would dilute the compressed gas, is permitted to enter the crank-case. Also the feature of expanding chlorine into low-pressure gas in the coil 18 is of advantage as it aids in keeping cool the bearings of the compressor and reduces the final pressure required in the liquefying coil 54%.

The water from waste 47 may, if desired, be used in the preliminary cooler 5 where the trap 38 is made sufiiciently deep to more than counterbalance the gas pressure in the crankcase, so that no chlorine gas can get back into the tower 13.

When the container 65 has been filled the valves 59 and 62 are closed and valve 69 opened for a moment to relieve the gas in these connections.

The pipe 341, which is preferably equipped with a gauge 34* and a valve 34 operates to equalize the pressure in the top of the chamber 30 to efiect free gravity flow of the acid therefrom.

The pipe 20 is preferabl e ui ed with a valve 20 by means of whizh the gressure of chlorine gas in the crank-case may be regulated.

In the arrangement shown in Figs. 3 and 4, the portions of the apparatus interposed etween the cooling apparatus Hand the pipe 61 in Fig. 1, are omitted and a chlorine-gas liquefying apparatus substituted for the apparatus 44 from which the liquefied chlorine may be charged directly into the shipping containers, such as the containers 65. The liquefying apparatus referred to comprises a tank 100 having a valved vent-pipe 100 and valved drain-pipe 100 the latter for the acid, into which the pipe 101, corresponding to the pipe 24 and prefer to employ sulphuric acid for.

through which the compressed chlorine gas containing some of the sulphuric acid, is forced by the operation of-the compressor 23, opens, this pipe extending downwardly in the tank 100 to a point closely adjacent the bottom thereof and preferably having branches 102 radiating therefrom and containing downwardly directed openings 102 along their lower sides through which the gas forced through the pipe 101, discharges into the lower portion of the tank 100 and into a body of sulphuric acid therein, and represented at 103. A coil 104 for a condensing medium is located in the tank 100*, this coil being submerged in the body 103 of acid. One end of this coil is connected with a pipe 105 which corresponds to the pipe-4C6 (Fi 1), and through which cooling water is supplied to the coil, as by connecting the pipe 105 with the pipe 53 of Fig. 1, the other end of the coil 104 being connected with a pipe 106 corresponding with the pipe 47 of Fig. 1. for conducting the cooling water away from the coil 10 1. The pipe represented at 106 corresponds with the pipe 20 of Fig. 1, and a pipe represented at 107 is provided for charging the sulphuric acid into the tank 100. in this particular apparatus, the compressed chlorine gas discharges into the body 103 of acid entering it, preferably in fine streams through the openings 102 in the branch pipes 102. In its passage upwardly through the relatively cold acid, the chlorine gas is condensed and floats on the top or" the body 103 of acid, the condensed chlorine gas passing from the tank through a pipe 108 having a flexible section 109 opening into a valve coupling 110 communicating with the inlet of the shipping container 65 and carried thereby.

it will be understood that while certain particular forms of apparatus are described and shown, I do not intend to limit the invention thereto as the same may be variously modified and altered without departing from N1 the spirit of my invention.

Furthermore, while It have described and claimed my improved apparatus as employed in the manufacture of liquefied chlorine, it will be readily understood that it may be used for the liquefaction of other gases, it being my intention to cover the use of the apparatus with all gases to which it is applicable.

What I claim as new and desire to secure by Letters Patent is:

1. In apparatus for liquefying chlorine gas, the combination or" a compressor for compressing the gas, means for effecting the introduction into the gas, for commingling therewith, of a substance condensable at a higher temperature than that at which the gas under the same pressure condenses, and means for cooling the mixture of the gas and the said substance operating to condense the gas and separate the liquefied gas from the said other substance in condensed condition.

2. In apparatus for liquefying chlorine gas, the combination of a compressor for the gas, a condenser, means for eifecting the introduction into the gas, for comminglin therewith, prior to the condensing thereo sulphuric acid, means for separating the sulphuric acid from the gas, and means Whereby gas is dried by the acid so separated.

In apparatus for liquefying chlorine gas, the combination of a compressor for the gas, means for effecting the introduction of sulphuric acid into the gas while being compressed in the compressor for admixture therewith in finely divided condition, condensing means, and means for separating the sulphuric acid from the condensed gas.

4. In apparatus for liquefying chlorine gas, the combination of a compressor for gas adapted in its operation to cause the gas being compressed to be commingled with sulphuric acid in finely divided condition, condensing means, means for separating the sulphuric acid from the condensed chlorine gas and means for subjecting the gas before it enters the compressor, to the cooling action of gas compressed by the compressor.

5. In apparatus for liquefying chlorine gas, the combination of a compressor for compressing gas, means for supplying sulphuric acid to the compressor, means for subjecting the gas before entering the compressor to the dryin action of sulphuric acid, means for supp ying said last-named means with sulphuric acid from the compressor, and means for. coolin the crankcasfi of the compressor to cool t e sulphuric ac1 6. In apparatus for liquefying chlorine gas, the combination of a course through WhlCh the chlorine passes, drying means for the gas, compressing means and condensing means in said course for compressing and acid, means for cooling the compressed gas and the sulphuric acid commingled therewith, means for separating the sulphuric acid and a portion of the compressed gas from the main body of compressed gas, and means for subjecting other chlorine gas prior to its introduction into the compressing means, to the cooling action of the separated sulphuric acid and the chlorine commingled therewith.

8. In apparatus .for liquefying chlorine gas, the combination of means for com pressing the gas in the presence of sulphuri acid, means for cooling the compressed gas and the sulphuric acid commingled therewith, means for separating the sulphuric acid and a portion of the compressed gas from the main body of compressed gas, and means for causing the separated sulphuric acid and the chlorine commingled therewith to become commingled-with other chlorine gas prior to the compressing of the latter.

9.-In=apparatus for liquefying chlorine gas, the combination of means for compressingthe as in the presence of sulphuric acid, means or cooling the compressed gas and the sulphuric acid commingled therewith, means for separating the sulphuric acid and a portion of the compressed gas from the main body of compressed gas, a course through which the gas passes and in which the compressing means is located, and means for conveying the separated sulphuric acid and the chlorine commingled therewith, into said course.

WILLIAM M. J EWELL. 

